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HMT continuous synthesis apparatus and method

A technology of chemical synthesis and transfer kettle, which is applied in the field of organic chemical industry, can solve the problems of poor heat and mass transfer effect and low production capacity, and achieve the effects of increased production capacity, high degree of automation and good safety

Active Publication Date: 2016-03-30
TIANMEN DEYUAN CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Although the above method is used for batch reaction, the operation is simple and the equipment investment is small, but the disadvantages of poor heat and mass transfer effect and low production capacity are also obvious.

Method used

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  • HMT continuous synthesis apparatus and method
  • HMT continuous synthesis apparatus and method

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preparation example Construction

[0027] A continuous synthesis method of HMT, comprising the steps of:

[0028] (I) Raw material liquid mixing stage: Put the reaction raw materials p-cymene, 2,3-dimethyl-1-butene, chloro-tert-butane and cyclohexane into the raw material storage tank respectively, open the valve and enter the mixing Kettle mix evenly;

[0029] (II) Mixed liquid reaction stage: the mixture is pumped into the tubular reactor and contacted with the aluminum chloride catalyst filled in the reactor, Friedel-Crafts alkylation reaction occurs under the action of the catalyst, and the reaction liquid flows out of the tubular reactor , into the transfer tank, the transfer tank is stirred to further stir the reaction solution evenly, and the reaction solution is collected into the washing tank by the overflow method;

[0030] (Ⅲ) Post-treatment stage: add water to the water washing kettle to quench, then wash with water and alkali, and carry out rectification, desolventization and recrystallization on ...

Embodiment 1

[0036]Add 804kg of p-cymene, 252kg of 2,3-dimethyl-1-butene, 416kg of chlorobutane and 1260kg of cyclohexane into the mixing tank and stir for 0.5-1h. During the stirring process, 80 kg of aluminum trichloride was charged into the tubular reactor. After the filling is completed, adjust the temperature of the tubular reactor to 10-15°C, start feeding through the centrifugal pump, and control the feeding speed at 0.7-2.5mL / s. Control the temperature in the transfer tank at 10-30°C, and start stirring when the reaction liquid flows into the transfer tank. After reacting for 4-6 hours, start sampling through the monitoring port every 30 minutes for monitoring, and replace the catalyst after the HMT content drops. The reaction liquid flows out through the overflow port. When the amount of reaction liquid in the washing kettle reaches 1800L, start to add 700L water to quench the reaction, and then wash with 500L sodium hydroxide solution and 600L water. During the process, keep the...

Embodiment 2

[0038] Add 402kg of p-cymene, 168kg of 2,3-dimethyl-1-butene, 222kg of chlorobutane and 1008kg of cyclohexane into the mixing tank and stir for 0.5-1h. During the stirring process, 60 kg of aluminum trichloride was charged into the tubular reactor. After the filling is completed, adjust the temperature of the tubular reactor to 15-20°C, start feeding through the centrifugal pump, and control the feeding speed at 2-4.5mLs. Control the temperature in the transfer tank at 15-20°C, and start stirring when the reaction liquid flows into the transfer tank. After reacting for 3-5 hours, start sampling through the monitoring port every 30 minutes for monitoring, and replace the catalyst after the HMT content drops. The reaction liquid flows out through the overflow port. When the amount of reaction liquid in the washing kettle reaches 1800L, start to add 700L water to quench the reaction, and then wash with 500L sodium hydroxide solution and 600L water. During the process, keep the i...

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Abstract

The present invention provides an HMT continuous synthesis apparatus and method. The method comprises: taking p-cymene, 2,3-dimethyl-1-butylene, tert-butylchloride cyclohexane as raw materials to prepare a liquid mixture; stirring the mixture uniformly and then placing the mixture into a tubular reactor containing aluminium trichloride; obtaining an HMT reaction liquid in the tubular reactor; carrying out heat insulation while stirring in a transfer kettle and then overflowing the liquid into a hydrolysis kettle; after water washing and alkaline washing, obtaining an HMT crude product by rectification; and obtaining HMT with high purity degree by recrystallization. According to the method provided by the present invention, the process safety is good, the reaction conditions are easy to control, and the product quality is stable, so that HMT continuous large-scale production can be achieved.

Description

technical field [0001] The invention relates to the technical field of organic chemical industry, more specifically to the key precursor 1,1,3,4,4,6-hexamethyl-1,2,3,4-tetrahydrogenation of high-grade artificial musk musk Continuous synthesis device and method of naphthalene. Background technique [0002] 1,1,3,4,4,6-Hexamethyl-1,2,3,4-tetrahydronaphthalene (HMT) is an important intermediate in the synthesis of tuna musk. Tuna musk is a polycyclic musk with a tetralin structure. It has excellent acid, alkali and light resistance, no irritation and allergy to the skin, and has a strong musk powdery fragrance. It is widely used in high-end cosmetics and washing products. After the toxicity problem of nitro musk was exposed, about 50% of synthetic musks on the market mainly rely on polycyclic musks, the most representative of which is tona musk. At present, there are only a handful of manufacturers producing Tuna musk, and most of them mainly rely on imports, which are far fr...

Claims

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Application Information

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IPC IPC(8): C07C2/72C07C13/48
CPCC07C2/72C07C13/48
Inventor 黎明刘升杜晓华黎继俭
Owner TIANMEN DEYUAN CHEM TECH CO LTD
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